Lithium Hydroxide → HCID 21017824、化合物

HRID 644939

反応式

HRID 644939 の反応式
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C@@H:8]2[CH2:13][CH2:12][C:11](=[O:14])[CH2:10][C@H:9]2[C:15]([O:17]C)=[O:16])=[CH:4][CH:3]=1.[OH-].[Li+].Cl.[Cl-].[Na+].O>O1CCCC1>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([C@@H:8]2[CH2:13][CH2:12][C:11](=[O:14])[CH2:10][C@H:9]2[C:15]([OH:17])=[O:16])=[CH:6][CH:7]=1

参加物

5

反応物 3

HCID 3939Lithium HydroxideHCID 68520286Methyl trans-2-(4-chlorophenyl)-5-oxocyclohexanecarboxylateHCID 131718760Hydrochloric acid brine

生成物 1

HCID 21017824HCID 21017824、化合物

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

A stirred mixture of 0.435 g (1.63 mmol) of methyl trans-2-(4-chlorophenyl)-5-oxocyclohexanecarboxylate (described in Step B of Example 1) and 1 N lithium hydroxide (3.26 mL, 3.26 mmol) in tetrahydrofuran (3.3 mL) was heated at reflux for approximately 1 h. After cooling to room temperature, the reaction mixture was poured into 1 N hydrochloric acid/brine (1:1) and extracted three times with methylene chloride. The combined organic extracts were washed with brine, dried (MgSO4) and concentrated in vacuo. The residual crude title compound was used without further purification in the subsequent reaction.

後処理

  1. temperaturewas heated
  2. temperatureat reflux for approximately 1 h
  3. extractionextracted three times with methylene chloride
  4. washThe combined organic extracts were washed with brine
  5. dry with materialdried (MgSO4)
  6. concentrationconcentrated in vacuo
  7. customThe residual crude title compound was used without further purification in the subsequent reaction

出典と根拠

ORDレコード
ord-1efd9cc470724fba99bfaf4fda84b551
出典データセット
uspto-grants-2010_04
特許番号
US07700778B2

関連ノート

読み込み中…